US8932975B2 - Catalyst systems and methods of making and using same - Google Patents
Catalyst systems and methods of making and using same Download PDFInfo
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- US8932975B2 US8932975B2 US12/876,954 US87695410A US8932975B2 US 8932975 B2 US8932975 B2 US 8932975B2 US 87695410 A US87695410 A US 87695410A US 8932975 B2 US8932975 B2 US 8932975B2
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- metallocene
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- 0 C*C(*1)C1C1(C2)C2CCC1 Chemical compound C*C(*1)C1C1(C2)C2CCC1 0.000 description 19
- CRSOQBOWXPBRES-UHFFFAOYSA-N CC(C)(C)C Chemical compound CC(C)(C)C CRSOQBOWXPBRES-UHFFFAOYSA-N 0.000 description 4
- LRVAPDYYLHIDPS-UHFFFAOYSA-F CC1=CC(C)=C(N2CCCCCN(C3=C(C)C=C(C)C=C3C)[Zr]2(CC2=CC=CC=C2)CC2=CC=CC=C2)C(C)=C1.COCCN1CC2=CC(C(C)(C)C)=CC(C(C)(C)C)=C2O[Zr](CC2=CC=CC=C2)(CC2=CC=CC=C2)OC2=C(C=C(C(C)(C)C)C=C2C(C)(C)C)C1.COCCN1CC2=CC(C(C)(C)C)=CC(C(C)(C)C)=C2O[Zr](Cl)(Cl)OC2=C(C=C(C(C)(C)C)C=C2C(C)(C)C)C1.COCCN1CCN(C2=C(C)C=C(C)C=C2C)[Zr](Cl)(Cl)N(C2=C(C)C=C(C)C=C2C)CC1 Chemical compound CC1=CC(C)=C(N2CCCCCN(C3=C(C)C=C(C)C=C3C)[Zr]2(CC2=CC=CC=C2)CC2=CC=CC=C2)C(C)=C1.COCCN1CC2=CC(C(C)(C)C)=CC(C(C)(C)C)=C2O[Zr](CC2=CC=CC=C2)(CC2=CC=CC=C2)OC2=C(C=C(C(C)(C)C)C=C2C(C)(C)C)C1.COCCN1CC2=CC(C(C)(C)C)=CC(C(C)(C)C)=C2O[Zr](Cl)(Cl)OC2=C(C=C(C(C)(C)C)C=C2C(C)(C)C)C1.COCCN1CCN(C2=C(C)C=C(C)C=C2C)[Zr](Cl)(Cl)N(C2=C(C)C=C(C)C=C2C)CC1 LRVAPDYYLHIDPS-UHFFFAOYSA-F 0.000 description 1
- QCIKZIGWGGEMBN-UHFFFAOYSA-F COCCN1CC2=CC(C(C)(C)C)=CC(C(C)(C)C)=C2O[Zr](CC2=CC=CC=C2)(CC2=CC=CC=C2)OC2=C(C=C(C(C)(C)C)C=C2C(C)(C)C)C1.COCCN1CC2=CC(C(C)(C)C)=CC(C(C)(C)C)=C2O[Zr](Cl)(Cl)OC2=C(C=C(C(C)(C)C)C=C2C(C)(C)C)C1.COCCN1CCN(C2=C(C)C=C(C)C=C2C)[Zr](Cl)(Cl)N(C2=C(C)C=C(C)C=C2C)CC1 Chemical compound COCCN1CC2=CC(C(C)(C)C)=CC(C(C)(C)C)=C2O[Zr](CC2=CC=CC=C2)(CC2=CC=CC=C2)OC2=C(C=C(C(C)(C)C)C=C2C(C)(C)C)C1.COCCN1CC2=CC(C(C)(C)C)=CC(C(C)(C)C)=C2O[Zr](Cl)(Cl)OC2=C(C=C(C(C)(C)C)C=C2C(C)(C)C)C1.COCCN1CCN(C2=C(C)C=C(C)C=C2C)[Zr](Cl)(Cl)N(C2=C(C)C=C(C)C=C2C)CC1 QCIKZIGWGGEMBN-UHFFFAOYSA-F 0.000 description 1
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- Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
Abstract
where M1 is Ti, Zr or Hf, X1 and X2 are each independently F, Cl, Br, I, methyl, benzyl, phenyl, H, BH4, a hydrocarbyloxide group having up to 20 carbon atoms, a hydrocarbylamino group having up to 20 carbon atoms, a trihydrocarbylsilyl group having up to 20 carbon atoms, OBR′2 wherein R′ may be an alkyl group having up to 12 carbon atoms or an aryl group having up to 12 carbon atoms, and SO3R″ wherein R″ may be an alkyl group having up to 12 carbon atoms or an aryl group having up to 12 carbon atoms, and Cp1 and Cp2 are each independently a substituted or unsubstituted cyclopentadienyl group, or a substituted or unsubstituted indenyl group, where any substituent on Cp1 and Cp2 is H, a hydrocarbyl group having up to 18 carbon atoms or a hydrocarbylsilyl group having up to 18 carbon atoms, (b) a second metallocene complex, (c) a non-group 4 metallocene transition-metal complex, (d) an activator or activator-support, and (e) an optional cocatalyst.
Description
where M1 is Ti, Zr or Hf, X1 and X2 are each independently F, Cl, Br, I, methyl, benzyl, phenyl, H, BH4, a hydrocarbyloxide group having up to 20 carbon atoms, a hydrocarbylamino group having up to 20 carbon atoms, a trihydrocarbylsilyl group having up to 20 carbon atoms, OBR′2 wherein R′ may be an alkyl group having up to 12 carbon atoms or an aryl group having up to 12 carbon atoms, and SO3R″ wherein R″ may be an alkyl group having up to 12 carbon atoms or an aryl group having up to 12 carbon atoms, and Cp1 and Cp2 are each independently a substituted or unsubstituted cyclopentadienyl group, or a substituted or unsubstituted indenyl group, where any substituent on Cp1 and Cp2 is H, a hydrocarbyl group having up to 18 carbon atoms or a hydrocarbylsilyl group having up to 18 carbon atoms, (b) a second metallocene complex, (c) a non-group 4 metallocene transition-metal complex, (d) an activator or activator-support, and (e) an optional cocatalyst.
where M1 is Ti, Zr, or Hf;
X1 and X2 are each independently F, Cl, Br, I, methyl, benzyl, phenyl, H, BH4, a hydrocarbyloxide group having up to 20 carbon atoms, a hydrocarbylamino group having up to 20 carbon atoms, a trihydrocarbylsilyl group having up to 20 carbon atoms, OBR′2 wherein R′ may be an alkyl group having up to 12 carbon atoms or an aryl group having up to 12 carbon atoms, and SO3R″, wherein R″ may be an alkyl group having up to 12 carbon atoms or an aryl group having up to 12 carbon atoms; and Cp1 and Cp2 are each independently a substituted or unsubstituted cyclopentadienyl group, or a substituted or unsubstituted indenyl group, where any substituent on Cp1 and Cp2 is H, a hydrocarbyl group having up to 18 carbon atoms or a hydrocarbylsilyl group having up to 18 carbon atoms.
where M2 is Ti, Zr or Hf; X3 and X4 are independently F, Cl, Br, I, methyl, phenyl, benzyl, H, BH4, a hydrocarbyloxide group having up to 20 carbon atoms, a hydrocarbylamino group having up to 20 carbon atoms, a trihydrocarbylsilyl group having up to 20 carbon atoms, OBR′2 wherein R′ may be an alkyl group having up to 12 carbon atoms or an aryl group having up to 12 carbon atoms, or SO3R″ wherein R″ may be an alkyl group having up to 12 carbon atoms or an aryl group having up to 12 carbon atoms; R1 and R2 are independently hydrogen or a hydrocarbyl group having up to 18 carbon atoms; Cp3 is a substituted or unsubstituted cyclopentadienyl group, a substituted or unsubstituted indenyl group, a substituted or unsubstituted fluorenyl group, where any substituent on Cp3 is H, a hydrocarbyl group having up to 18 carbon atoms or a hydrocarbylsilyl group having up to 18 carbon atoms; and E represents a bridging group which may comprise (i) a cyclic or heterocyclic moiety having up to 18 carbon atoms, (ii) a group represented by the general formula EAR3AR4A, wherein EA is C or Si, and R3A and R4A are independently H or a hydrocarbyl group having up to 18 carbon atoms, (iii) a group represented by the general formula —CR3BR4B—CR3CR4C—, wherein R3B, R4B, R3C, and R4C are independently H or a hydrocarbyl group having up to 10 carbon atoms, (iv) a group represented by the general formula —SiR3DR4D—SiR3ER4E—, wherein R3D, R4D, R3E, and R4E are independently H or a hydrocarbyl group having up to 10 carbon atoms, and wherein at least one of R3A, R3B, R4A, R4B, R3C, R4C, R3D, R4D, R3E, R4E, or the substituent on Cp3 is (1) a terminal alkenyl group having up to 12 carbon atoms or (2) a dinuclear compound wherein each metal moiety has the same structural characteristic as MTE-B. Nonlimiting examples of compounds suitable for use in this disclosure as MTE-B are represented by structures (14)-(29):
M(OR)yClz Formula I
M(NR2)yClz Formula II
where y+z=valence of the metal, R is a hydrocarbon group having up to 12 carbon atoms and M is titanium, vanadium, zirconium, hafnium, chromium, molybdenum, tungsten, iron, cobalt, nickel, copper, or a lanthanides complex. Nonlimiting examples of compounds suitable for use as CAT-3 in this disclosure include TiCl4, Zr(CH2Ph)4, Hf(CH2Ph)4, Zr(NMe2)4, CrCl3, VCl5, Ti(OBu)Cl3, Ti(OBu)3Cl, Ti(O-i-Pr)2Cl2, VOCl3, Cp2Cr where Cp is a cyclopentadienyl group, (EtCp)2Cr, CpCr(Py)Me2, CpCr(Py)Cl2 and compounds represented by structures (30)-(33), where Bn is benzyl:
Al(X5)p(X6)q
where X5 is a halide, hydrocarbyloxide group, hydrocarbylamino group or combinations thereof; X6 is a hydrocarbyl group having up to 18 carbon atom; p ranges from 0 to 2; and q is 3−p
wherein each R is independently a linear or branched alkyl having from 1 to 10 carbon atoms, and p′ ranges from 3 to 20 are encompassed by this disclosure. The AlRO moiety shown here also constitutes the repeating unit in a linear aluminoxane. Thus, linear aluminoxanes having the formula:
wherein R is a linear or branched alkyl having from 1 to 10 carbon atoms and, q′ is an integer from 1 to 50, are also encompassed by this disclosure. Further, aluminoxanes suitable for use in this disclosure can have cage structures of the formula Rt 5r+αRb r−αAl4rO3r, wherein Rt is a terminal linear or branched alkyl group having from 1 to 10 carbon atoms; Rb is a bridging linear or branched alkyl group having from 1 to 10 carbon atoms; r is 3 or 4; and α is equal to nAl(3)−nO(2)+nO(4), wherein nAl(3) is the number of three coordinate aluminum atoms, nO(2) is the number of two coordinate oxygen atoms, and nO(4) is the number of 4 coordinate oxygen atoms.
where Ni is the number of molecules of molecular weight Mi. All molecular weight averages are expressed in gram per mole (g/mol) or Daltons and are determined by gel permeation chromatography. The number average molecular weight is the common average of the molecular weights of the individual polymers calculated by measuring the molecular weight of n polymer molecules, summing the weights, and dividing by n.
The z-average molecular weight is a higher order molecular weight average which is calculated according to equation (3)
M z =Σn i M i 3 /Σn i M i 2 (kg mol−1) (3)
where ni is the amount of substance of species i and Mi is the molar mass of species.
TABLE 1 | |||||
MTEA/MTE-B | |||||
Sample No. | MTE-A | MTE-B | (mg/mg) | Activator-Support (150 mg) | TIBAL (mmol) |
2 | |
Compound 16 | 1/0.7 | sulfated alumina | 0.5 |
3 | |
Compound 16 | 1/0.7 | Ti-containing sulfated alumina | 0.5 |
4 | |
Compound 15 | 1.75/0.2 | Sulfated alumina | 0.7 |
5 | |
Compound 15 | 1.75/0.2 | Ti-containing sulfated alumina | 0.7 |
6 | |
Compound 18 | 1/0.8 | Sulfated alumina | 0.5 |
7 | |
Compound 18 | 1/0.8 | Ti-containing sulfated alumina | 0.5 |
*The compound numbers correspond to the structure numbers presented in the disclosure such that for |
TABLE 2 | ||||||
1-hexene | H2/C2 | Time | Temp. | Pressure | Solid PE | |
Resin No. | (g) | (ppm) | (min.) | (° C.) | (psi) | (g) |
|
0 | 350 | 30 | 95 | 420 | 271.0 |
R3 | 8.0 | 350 | 30 | 95 | 420 | 213.0 |
R4 | 8.0 | 350 | 30 | 92 | 400 | 169.0 |
R5 | 8.0 | 350 | 30 | 92 | 400 | 176.0 |
R6 | 8.0 | 350 | 45 | 95 | 420 | 224.0 |
R7 | 8.0 | 350 | 45 | 95 | 420 | 191.0 |
TABLE 3a | |||||||||
Resin | MI | HLMI | HLMI/ | ||||||
No. | Mn/1000 | Mw/1000 | Mz/1000 | Mw/Mn | Mz/Mw | η0 | g/10 min | g/10 min | MI |
R1* | 8.1 | 264.1 | 1069.1 | 32.6 | 3.8 | 1.52E+05 | 0.060 | 7.4 | 123 |
R2 | 8.1 | 125.4 | 435.3 | 15.4 | 3.5 | 1.43E+04 | 0.670 | 41.6 | 62 |
R3 | 8.1 | 258.2 | 2003.6 | 31.9 | 8.1 | 4.70E+05 | 0.052 | 10.1 | 193 |
*R1 was produced from |
TABLE 3b | ||||||||||
Fluff | ||||||||||
Resin | Density | MI | HLMI | HLMI/ | ||||||
No. | (g/cc) | Mn/1000 | Mw/1000 | Mz/1000 | Mw/Mn | Mz/Mw | η0 | g/10 min | g/10 min | MI |
R1 | 0.9516 | 8.1 | 264.1 | 1069.1 | 32.6 | 3.8 | 1.52E+05 | 0.060 | 7.4 | 123 |
R4 | 0.9519 | 9.3 | 206.0 | 689.6 | 22.3 | 3.3 | 7.91E+04 | 0.083 | 15.4 | 185 |
R5 | 0.952 | 14.1 | 262.2 | 1577.3 | 18.6 | 6.0 | 1.65E+05 | 0.029 | 16.3 | 563 |
R6 | 0.9521 | 9.8 | 252.0 | 1322.0 | 25.9 | 5.2 | 1.54E+05 | 0.090 | 15.6 | 173 |
R7 | 0.951 | 12.3 | 347.0 | 2420.1 | 28.3 | 7.0 | 7.45E+05 | 0.032 | 25.8 | 805 |
Claims (29)
M(NR2)yClz Formula II
Al(X5)p(X6)q
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